一里坪硫酸镁亚型盐湖钾镁混盐转化-浮选中物相行为

doi:10.11949/j.issn.0438-1157.20181286

化工学报 ›› 2019, Vol. 70 ›› Issue (5): 1832-1841.DOI: 10.11949/j.issn.0438-1157.20181286

一里坪硫酸镁亚型盐湖钾镁混盐转化-浮选中物相行为

时历杰^1,²(),王敏^1,²()

1. 中国科学院青海盐湖研究所，中国科学院盐湖资源综合高效利用重点实验室，青海西宁 810008
2. 青海省盐湖资源化学重点实验室，青海西宁 810008

收稿日期:2018-10-31 修回日期:2019-02-18 出版日期:2019-05-05 发布日期:2019-05-05
通讯作者: 王敏
作者简介:<named-content content-type="corresp-name">时历杰</named-content>（1984—），男，硕士，助理研究员，<email>lijieshi@isl.ac.cn</email>|王敏（1966—），女，学士，研究员，<email>marliy001@163.com</email>
基金资助:
国家自然科学基金项目(415030610);青海盐湖研究所引导基金项目(Y560311147);青海省重点研发与转化计划项目(2017-GX-145)

Phase behavior of K-Mg mixed salt during transformation-flotation from Yiliping magnesium sulfate-type salt lake

Lijie SHI^1,²(),Min WANG^1,²()

1. Key Laboratory of Comprehensive and Highly Efficient Utilization of Salt Lake Resources, Qinghai Institute of Salt Lakes, Chinese Academy of Sciences, Xining 810008, Qinghai, China
2. Key Laboratory of Salt Lake Resources Chemistry of Qinghai Province, Xining 810008, Qinghai, China

Received:2018-10-31 Revised:2019-02-18 Online:2019-05-05 Published:2019-05-05
Contact: Min WANG

摘要/Abstract

摘要：

加水比例及物相行为研究对硫酸镁亚型盐湖钾镁混盐转化制备软钾镁矾工艺具有重要意义。以柴达木盆地一里坪盐湖钾镁混盐为对象，采用“转化-浮选”法制备钾盐镁矾，研究了钾镁混盐初始及转化产生的物相行为。结果表明，初始物相光卤石、水氯镁石溶解速率最快，分解得到新物相氯化钾。初始物相钾盐镁矾及其转化得到的新物相软钾镁矾，溶解转化速率次之，加水比例高于0.40时，速率趋于平缓。初始物相氯化钠溶解速率始终最低。转化过程中，氯化钾只发生溶解行为，并未与软钾镁矾反应生成新物相硫酸钾。转化实验结果与理论计算结果吻合度高，相对误差低于4%，利用介稳相图理论计算能够指导钾镁混盐转化。同时，正浮选捕收剂对含钾物相的捕收吸附能力强于反浮选，钾的总收率达到66%。

关键词: 钾镁混盐, 溶解转化, 钾盐镁矾, 物相行为, 硫酸镁亚型, 介稳相平衡, 制备, 浮选

Abstract:

Study on water-salt mass ratio and phase behavior during the K-Mg mixed salt transformation from magnesium sulfate-type salt lake is important for preparing Pic (Picromerite). Pic was prepared from the K-Mg mixed salt of Yiliping salt lake in Qaidam Basin by means of transformation-flotation. Phase behavior was researched which was the initial and new produced by transformation. The results showed that the dissolution rate of the initial phase Car (Carnallite) and Bis (Bischofite) was the fastest, and the new phase KCl (Sylvite) was obtained by decomposition. The dissolution and transformation rate of the initial phase Kai (Kainite) and the new phase Pic transformed from Kai was second, and while the water-salt mass ratio was higher than 0.40, the rate tended to be flat. The dissolution rate of the initial phase NaCl (Halite) was always the lowest. During the transformation, KCl only dissolved, didn’t react with Pic to form a new phase SOP (potassium sulfate). Experimental results of the K-Mg mixed salt transformation were in good agreement with theoretical calculation results, the relative error was less than 4% between them, the theoretical calculations of the metastable phase diagram could be used to guide the K-Mg mixed salt transformation better. Finally, the obverse flotation collector had stronger capacity for collecting and adsorbing the K-containing phase than the reverse, the total yield of K had been reached 66%.

Key words: K-Mg mixed salt, dissolution and transformation, kainite, phase behavior, magnesium sulfate type, metastable phase equilibria, preparation, flotation

中图分类号:

时历杰, 王敏. 一里坪硫酸镁亚型盐湖钾镁混盐转化-浮选中物相行为[J]. 化工学报, 2019, 70(5): 1832-1841.

Lijie SHI, Min WANG. Phase behavior of K-Mg mixed salt during transformation-flotation from Yiliping magnesium sulfate-type salt lake[J]. CIESC Journal, 2019, 70(5): 1832-1841.

图/表 12

参考文献 31

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Name	No.	Chemical composition/%					Phase composition/%
Name	No.	Na⁺	K⁺	Mg²⁺	Cl^-	SO₄ ^2-	NaCl	Kai	Car	Bis
K-Mg mixed salt	S0	10.86	10.18	6.65	29.07	22.09	27.61	56.21	8.45	2.69

Name	No.	Chemical composition/%					Phase composition/%
Name	No.	Na⁺	K⁺	Mg²⁺	Cl^-	SO₄ ^2-	NaCl	Kai	Car	Bis
K-Mg mixed salt	S0	10.86	10.18	6.65	29.07	22.09	27.61	56.21	8.45	2.69

Name	No.	Quantity/g	Chemical composition/%					Phase composition/%
Name	No.	Quantity/g	Na⁺	K⁺	Mg²⁺	Cl^-	SO₄ ^2-	NaCl	Kai	Car	Bis	Pic
K-Mg mixed salt	S0	100.00	10.86	10.18	6.65	29.07	22.09	27.61	56.21	8.45	2.69
water	W	60.32
water-salt mass ratio	m	m=0.6032
mother liquid after transformation	L1	104.16	2.85	3.05	4.30	16.22	4.71
solid after transformation	S1	56.16	14.07	12.47	3.88	21.70	30.64	35.78				64.22
solid yield/%			72.76	68.79	32.77	41.92	77.90

Name	No.	Quantity/g	Chemical composition/%					Phase composition/%
Name	No.	Quantity/g	Na⁺	K⁺	Mg²⁺	Cl^-	SO₄ ^2-	NaCl	Kai	Car	Bis	Pic
K-Mg mixed salt	S0	100.00	10.86	10.18	6.65	29.07	22.09	27.61	56.21	8.45	2.69
water	W	60.32
water-salt mass ratio	m	m=0.6032
mother liquid after transformation	L1	104.16	2.85	3.05	4.30	16.22	4.71
solid after transformation	S1	56.16	14.07	12.47	3.88	21.70	30.64	35.78				64.22
solid yield/%			72.76	68.79	32.77	41.92	77.90

Name	No.	Quantity/g	Chemical composition/%
Name	No.	Quantity/g	Na⁺	K⁺	Mg²⁺	Cl^-	SO₄ ^2-
K-Mg mixed salt	S0	200	10.86	10.18	6.65	29.07	22.09
m=0.30
water	W	60
mother liquid after transformation	L2	100	1.90	2.65	5.28	16.63	5.57
solid after transformation	S2	160	12.96	10.48	4.88	25.60	24.54
solid yield/%			91.59	86.35	59.66	71.12	87.57
m=0.40
water	W	80
mother liquid after transformation	L3	145	1.94	2.85	5.00	16.15	5.44
solid after transformation	S3	135	13.02	10.71	4.11	22.94	25.52
solid yield/%			86.19	77.77	43.35	56.94	81.37
m=0.50
water	W	100
mother liquid after transformation	L4	170	2.40	2.86	4.72	16.05	5.44
solid after transformation	S4	130	13.38	10.78	3.94	22.90	25.75
solid yield/%			81.00	74.24	38.96	52.18	78.35
m=0.60
water	W	120
mother liquid after transformation	L5	200	2.37	2.84	4.57	15.52	5.48
solid after transformation	S5	120	14.41	11.42	3.84	22.59	28.70
solid yield/%			78.47	70.70	33.52	46.62	75.86

一里坪硫酸镁亚型盐湖钾镁混盐转化-浮选中物相行为

Phase behavior of K-Mg mixed salt during transformation-flotation from Yiliping magnesium sulfate-type salt lake

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No.	Salt molarity/(mol/L)				J?necke index(Mg²⁺+K₂ ²⁺+SO₄ ^2-=100 mol)
No.	c(Na₂Cl₂)	c(K₂Cl₂)	c(MgSO₄)	c(MgCl₂)	Mg²⁺	K₂ ²⁺	SO₄ ^2-	Na₂ ²⁺	H₂O
L2	0.5174	0.4236	0.7248	1.9907	70.28	10.96	18.76	13.39	1220.53
L3	0.5279	0.4556	0.7079	1.8636	68.85	12.20	18.95	14.13	1274.77
L4	0.6524	0.4572	0.7079	1.7196	67.57	12.72	19.70	18.16	1323.60
L5	0.6448	0.4540	0.7131	1.6373	66.82	12.91	20.27	18.33	1365.45
L1	0.7748	0.4876	0.6129	1.5986	66.77	14.72	18.50	23.39	1442.87

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Name	No.	Phase composition/%				J?necke index（Mg²⁺+K₂ ²⁺+SO₄ ^2-=100 mol）
Name	No.	NaCl	Kai	KCl	Pic	Mg²⁺	K₂ ²⁺	SO₄ ^2-
K-Mg mixed salt	S0	27.61	56.21	8.45(Car)	2.69(Bis)	43.17	20.54	36.29
solid after transformation	S2	32.94	35.71	0.93	22.05	34.02	22.70	43.28
	S3	33.10	17.67	0.62	38.94	29.58	23.96	46.46
	S4	34.01	13.77	0.57	42.64	28.54	24.27	47.19
	S5	36.63	2.54		56.72	26.21	24.23	49.56
	S1	35.78			64.22	25.00	25.00	50.00
KCl	A					0.00	100.00	0.00
Bis	C					100.00	0.00	0.00
Car	D					66.67	33.33	0.00
Kai	E					40.00	20.00	40.00
Pic	F					25.00	25.00	50.00

Name	No.	Phase composition/%				J?necke index（Mg²⁺+K₂ ²⁺+SO₄ ^2-=100 mol）
Name	No.	NaCl	Kai	KCl	Pic	Mg²⁺	K₂ ²⁺	SO₄ ^2-
K-Mg mixed salt	S0	27.61	56.21	8.45(Car)	2.69(Bis)	43.17	20.54	36.29
solid after transformation	S2	32.94	35.71	0.93	22.05	34.02	22.70	43.28
	S3	33.10	17.67	0.62	38.94	29.58	23.96	46.46
	S4	34.01	13.77	0.57	42.64	28.54	24.27	47.19
	S5	36.63	2.54		56.72	26.21	24.23	49.56
	S1	35.78			64.22	25.00	25.00	50.00
KCl	A					0.00	100.00	0.00
Bis	C					100.00	0.00	0.00
Car	D					66.67	33.33	0.00
Kai	E					40.00	20.00	40.00
Pic	F					25.00	25.00	50.00

Name	No.	Quantity/g	Chemical composition/%					Phase composition/%
Name	No.	Quantity/g	Na⁺	K⁺	Mg²⁺	Cl^-	SO₄ ^2-	NaCl	Kai	KCl	Pic
solid after transformation	S4-1	180	13.38	10.78	3.94	22.90	25.75	34.01	13.74	1.15	42.64
obverse flotation collector	Y1	0.12
collector-solid mass ratio	y1	y1=670 g(collector):1 t(solid)
obverse flotation bubbles	Pic1	105	1.46	17.40	5.82	3.98	42.03	3.71	10.10	1.11	79.79
obverse flotation tailings	A	75	30.11	1.48	0.54	46.70	3.60	76.54	1.72	0.071	6.10
bubbles yield/%			6.35	94.27	93.78		94.23	6.35	89.16	95.63	94.82
solid after transformation	S4-2	180	14.40	11.02	3.86	23.59	26.94	36.61	9.14	0.24	48.89
reverse flotation collector	Y2	0.12
collector-solid mass ratio	y2	y2=670 g(collector):1 t(solid)
reverse flotation bubbles	B	73	30.00	3.65	1.39	47.28	8.61	76.26	6.08	0.57	13.02
reverse flotation tailings	Pic2	107	2.70	16.67	5.63	5.83	40.47	6.86	10.26	0.75	76.39
tailings yield/%			11.65	87.00	85.58		87.32	11.65	71.21	65.85	89.58

Name	No.	Quantity/g	Chemical composition/%					Phase composition/%
Name	No.	Quantity/g	Na⁺	K⁺	Mg²⁺	Cl^-	SO₄ ^2-	NaCl	Kai	KCl	Pic
solid after transformation	S4-1	180	13.38	10.78	3.94	22.90	25.75	34.01	13.74	1.15	42.64
obverse flotation collector	Y1	0.12
collector-solid mass ratio	y1	y1=670 g(collector):1 t(solid)
obverse flotation bubbles	Pic1	105	1.46	17.40	5.82	3.98	42.03	3.71	10.10	1.11	79.79
obverse flotation tailings	A	75	30.11	1.48	0.54	46.70	3.60	76.54	1.72	0.071	6.10
bubbles yield/%			6.35	94.27	93.78		94.23	6.35	89.16	95.63	94.82
solid after transformation	S4-2	180	14.40	11.02	3.86	23.59	26.94	36.61	9.14	0.24	48.89
reverse flotation collector	Y2	0.12
collector-solid mass ratio	y2	y2=670 g(collector):1 t(solid)
reverse flotation bubbles	B	73	30.00	3.65	1.39	47.28	8.61	76.26	6.08	0.57	13.02
reverse flotation tailings	Pic2	107	2.70	16.67	5.63	5.83	40.47	6.86	10.26	0.75	76.39
tailings yield/%			11.65	87.00	85.58		87.32	11.65	71.21	65.85	89.58